CN104458631B - It is a kind of to repeatedly use the method that crucible determines carbon and sulfur in material - Google Patents
It is a kind of to repeatedly use the method that crucible determines carbon and sulfur in material Download PDFInfo
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- CN104458631B CN104458631B CN201310431260.XA CN201310431260A CN104458631B CN 104458631 B CN104458631 B CN 104458631B CN 201310431260 A CN201310431260 A CN 201310431260A CN 104458631 B CN104458631 B CN 104458631B
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Abstract
The invention discloses a kind of repeatedly use the method that crucible determines carbon and sulfur in material.The method is that carbon or sulfur content meet in the case that analytical error requires in measured and monitored the growth of standing timber material is guaranteed, reuses crucible and determines carbon content 5~6 times in material;Or sulfur content 2~3 times in reuse crucible measure material.The present invention, is corrected to INFRARED ABSORPTION carbon sulfur instrument using used crucible when next time uses by used crucible is deposited in exsiccator different region by access times, to guarantee the accuracy tested, precision;The reuse of crucible is realized, the learies of crucible are not only reduced;The usage amount of flux is decreased simultaneously, reduces energy consumption, experimentation cost and the pollution speed to environment, favorable environment protection.
Description
Technical field
The present invention relates to a kind of repeatedly use the method that crucible determines carbon and sulfur in material, belong to measuring for materials
Field.
Background technology
Carbon, sulfur content in experimental determination metal or other materials, mostly using infrared absorption spectrometry.Should
Porcelain crucible used in method, is commercially available 25 × 25mm crucibles, and after crucible is bought, needs are first placed on crucible in Muffle furnace
Calcination in 1000 DEG C~1200 DEG C temperature ranges naturally cooled to room temperature after 4 hours, was stored in standby in exsiccator.Before detection,
Also need to crucible is taken out from exsiccator, detecting instrument is carried out by software program and rule of operation on INFRARED ABSORPTION carbon sulfur instrument
Correction test, after instrumental correction is good, then carries out specimen test.After often being used once due to crucible, the working curve of instrument
Will change.In order to ensure the accuracy and elaboration of measure.Therefore test crucible only to use once in prior art, nothing
All pass into disuse by whether damaging, cause to waste.The Disabled slags that sample is formed after test in the crucible discarded simultaneously and crucible all can
Certain pollution is formed to the natural environment of surrounding.
The content of the invention
It is an object of the present invention to provide a kind of repeatedly use the method that crucible determines carbon and sulfur in material, reduce
The discarded amount of crucible, to save experimentation cost, while can also reduce the impact of discarded crucible and Disabled slags to the natural environment of surrounding.
Technical scheme:
A kind of to repeatedly use the method that crucible determines carbon and sulfur in material, the method is by the exsiccator of storage crucible
Inside it is divided into 6 regions, commercially available crucible is stored in standby in 0 region Jing after processing, when testing for the first time, takes and be stored in 0th area
Crucible in domain is tested, and after testing for the first time, used crucible is stored in standby in 1 region Jing after processing;Try for second
When testing, take the crucible being stored in 1 region and tested, used crucible is stored in 2 Jing after processing after second test
It is standby in region;By that analogy, every time used crucible to be stored in subsequent region standby, one can only be taken during test next time
The crucible in region is tested;INFRARED ABSORPTION carbon sulfur instrument should be carried out using last time used crucible before formal test every time
Correction test, in the case that carbon or sulfur content meet analytical error requirement in measured and monitored the growth of standing timber material is guaranteed, reuses crucible
Carbon content 5~6 times in measure material;Or sulfur content 2~3 times in reuse crucible measure material.
It is in preceding method, described process is carried out to commercially available crucible to be:Commercially available crucible is placed in Muffle furnace 1000~
Calcination in 1200 DEG C of temperature ranges naturally cooled to room temperature after 4 hours, was put into standby in 0 region in exsiccator.
It is in preceding method, described process is carried out to used crucible to be:By used crucible from INFRARED ABSORPTION carbon sulfur
After removing on instrument, cool down 10~20 minutes in being firstly placed on anti-scald cooler, then the grit of crucible outer wall blown clean with hair-dryer,
It is then placed in standby in exsiccator respective regions.
In preceding method, the correction test be weigh 0.2~0.5g of standard substance and the special tungsten particle of determination of carbon and sulfur 1.0~
1.5g is corrected test by formal test code to INFRARED ABSORPTION carbon sulfur instrument, and writes down standard substance used and determination of carbon and sulfur is special
With the consumption of tungsten particle.
In preceding method, the use of standard substance and determination of carbon and sulfur special tungsten particle when correction test is taken during the formal test
Amount is placed on corrected INFRARED ABSORPTION carbon sulfur instrument to be tested.
In preceding method, after the formal test, remove after crucible from INFRARED ABSORPTION carbon sulfur instrument, earthenware should be examined
Crucible, if there is slag to spill or rupture, discards this crucible or is used after processing to this crucible again.
Compared with prior art, the present invention is by depositing in exsiccator different area by access times by used crucible
Domain, when next time uses, is corrected to INFRARED ABSORPTION carbon sulfur instrument using used crucible, to guarantee the accuracy tested, essence
Density;The reuse of crucible is realized, the learies of crucible are not only reduced;The usage amount of flux is decreased simultaneously,
Reduce energy consumption, experimentation cost and the pollution speed to environment, favorable environment protection.
Specific embodiment
The present invention is described in further detail for structure example below, but not as any limitation of the invention.
Embodiment
A kind of to repeatedly use the method that crucible determines carbon and sulfur in material, the method is by the exsiccator of storage crucible
Inside it is divided into 6 regions, commercially available crucible is stored in standby in 0 region Jing after processing, when testing for the first time, takes and be stored in 0th area
Crucible in domain is tested, and after testing for the first time, used crucible is stored in standby in 1 region Jing after processing;Try for second
When testing, take the crucible being stored in 1 region and tested, used crucible is stored in 2 Jing after processing after second test
It is standby in region;By that analogy, every time used crucible to be stored in subsequent region standby, one can only be taken during test next time
The crucible in region is tested;INFRARED ABSORPTION carbon sulfur instrument should be carried out using last time used crucible before formal test every time
Correction test, in the case that carbon or sulfur content meet analytical error requirement in measured and monitored the growth of standing timber material is guaranteed, reuses crucible
Carbon content 5~6 times in measure material;Or sulfur content 2~3 times in reuse crucible measure material.It is described that commercially available crucible is entered
Row process is:Commercially available crucible is placed in Muffle furnace the calcination in 1000~1200 DEG C of temperature ranges to naturally cool to after 4 hours
Room temperature, is put into standby in 0 region in exsiccator.It is described process is carried out to used crucible to be:By used crucible from red
After removing on outer absorption carbon sulfur instrument, it is firstly placed on cooling down 10~20 minutes in anti-scald cooler, then with hair-dryer by crucible outer wall
Grit blows clean, and is then placed in standby in exsiccator respective regions.The correction test be weigh 0.2~0.5g of standard substance and
Special 1.0~the 1.5g of tungsten particle of determination of carbon and sulfur is corrected test to INFRARED ABSORPTION carbon sulfur instrument by formal test code, and writes down institute
With standard substance and the consumption of the special tungsten particle of determination of carbon and sulfur.Standard substance and carbon sulfur when correction test is taken during the formal test
The consumption for determining special tungsten particle is placed on corrected INFRARED ABSORPTION carbon sulfur instrument and is tested.After formal test, from INFRARED ABSORPTION
After crucible is removed on carbon sulfur instrument, crucible should be examined, if there is slag to spill or rupture, discard this crucible or this crucible is entered
Row is used after processing again.
When being embodied as, reacted crucible will be tested, and remove from INFRARED ABSORPTION carbon sulfur instrument and processed, be put into special
In exsiccator, respective regions are stand-by;Use standard substance(Sample)Correction linearity curve;Repeatedly use crucible to be tested, one
As can use crucible to determine carbon content 5~6 times, sulfur content 2~3 times can be determined with crucible.Measured and monitored the growth of standing timber material carbon, sulfur content meet
Analytical error is required.Concrete operation step is as follows:
1st, reacted crucible will be tested, is removed from INFRARED ABSORPTION carbon sulfur instrument, in being placed on anti-scald cooler, is cooled down 10min
~20min, is put into respective regions in special exsiccator after removing outer wall grit with hair-dryer(0~5)It is stand-by.
2nd, crucible is taken out from special exsiccator, on INFRARED ABSORPTION carbon sulfur instrument carry out school by software program and rule of operation
[wherein selection standard material is tested just(Sample)Weighed sample amount is 0.2g~0.5g, and the special tungsten particle of added determination of carbon and sulfur is
1.0g~1.5g.], correct to result of the test and analyzing in allowed band with standard value error.
3rd, after instrumental correction is good, carry out specimen test.Test crucible takes and correction test same area, alleged test portion
Amount and the special tungsten particle of added determination of carbon and sulfur and correction test consumption are about etc..
When the 4th, crucible is removed from INFRARED ABSORPTION carbon sulfur instrument every time, observe crucible:If there is slag to spill or rupture, discard
It is stand-by that this crucible, otherwise process crucible are placed in subsequent region in special exsiccator.
5th, tested by 1-4 step cycles.
Claims (1)
- It is 1. a kind of to repeatedly use the method that crucible determines carbon and sulfur in material, it is characterised in that:The method is will to deposit earthenware It is divided into 6 regions in the exsiccator of crucible, commercially available crucible is stored in standby in 0 region Jing after processing, when testing for the first time, takes The crucible being stored in 0 region is tested, and after testing for the first time, used crucible is stored in standby in 1 region Jing after processing With;When testing for second, take the crucible being stored in 1 region and tested, after second test at used crucible Jing It is stored in after reason standby in 2 regions;By that analogy, every time used crucible to be stored in subsequent region standby, during test next time The crucible that a region can only be taken is tested;Every time should be using last time used crucible to infrared suction before formal test Receive carbon sulfur instrument and be corrected test, in the case that in measured and monitored the growth of standing timber material is guaranteed, carbon or sulfur content meet analytical error requirement, Carbon content 5~6 times in reuse crucible measure material;Or sulfur content 2~3 times in reuse crucible measure material;To city Selling crucible and carrying out process is:By commercially available crucible be placed in Muffle furnace in 1000~1200 DEG C of temperature ranges after calcination 4 hours from Room temperature is so cooled to, is put into standby in 0 region in exsiccator;Process is carried out to used crucible is:By used crucible After removing from INFRARED ABSORPTION carbon sulfur instrument, cool down 10~20 minutes in being firstly placed on anti-scald cooler, then with hair-dryer by outside crucible The grit of wall blows clean, and is then placed in standby in exsiccator respective regions;Correction test be weigh 0.2~0.5g of standard substance and Special 1.0~the 1.5g of tungsten particle of determination of carbon and sulfur is corrected test to INFRARED ABSORPTION carbon sulfur instrument by formal test code, and writes down institute With standard substance and the consumption of the special tungsten particle of determination of carbon and sulfur;Standard substance and determination of carbon and sulfur when correction test is taken during formal test The consumption of special tungsten particle is placed on corrected INFRARED ABSORPTION carbon sulfur instrument and is tested;After formal test, from INFRARED ABSORPTION carbon sulfur After crucible is removed on instrument, crucible should be examined, if there is slag to spill or rupture, discard this crucible or to this crucible at Used after reason again.
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CN105466880A (en) * | 2015-12-26 | 2016-04-06 | 首钢总公司 | Sample pretreatment method for measuring contents of sulfur in dolomite and limestone |
CN108414470B (en) * | 2018-04-10 | 2020-11-13 | 中国航发北京航空材料研究院 | Method for measuring ultralow sulfur content in wrought superalloy |
CN112326584A (en) * | 2020-10-19 | 2021-02-05 | 本钢板材股份有限公司 | Method for detecting sulfur and carbon in steel |
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CN103266294A (en) * | 2013-03-07 | 2013-08-28 | 贵阳嘉瑜光电科技咨询中心 | Method of repeatedly using molybdenum crucible in HEM crystal growth |
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